関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | (2-Iodobenzoylamino)-(2-iodophenyl)-acetic Acid Methyl Ester | HCID 68839341 | — |
| 触媒 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 7-Oxo-6,7-dihydro-5H-dibenzo[c,e]azepine-5-carboxylic Acid Methyl Ester | HCID 68838469 | — |
反応手順
To a solution of (2-iodobenzoylamino)-(2-iodophenyl)-acetic acid methyl ester (3.4 g, 6.53 mmol) in DMF (300 mL) under argon is added PdCl2(dppf) (269 mg, 0.33 mmol) and KOAc (1.28 g, 13.06 mmol) and the mixture is heated at 110° C. for 18 h. Additional PdCl2(dppf) is added and heating is continued until all starting material is consumed. The solvent is removed under reduced pressure and the residue purified by flash chromatography using a gradient of 0-50% MeOH/methylene chloride as eluent to give the title compound as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08084448B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-f5e80b2965294fee9b2c92aaa0c2d7ed |
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| 出典メモ | uspto-grants-2011_12 |
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